CN103056347A - Method for controlling dendritic crystal orientation of oriented solidification structure by high-intensity magnetic field - Google Patents
Method for controlling dendritic crystal orientation of oriented solidification structure by high-intensity magnetic field Download PDFInfo
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Abstract
The invention relates to a method for controlling dendritic crystal orientation of a oriented solidification structure by a high-intensity magnetic field. The difference between preferred orientation and easy magnetization direction of a dendritic crystal during oriented solidification process is utilized, and the high-intensity magnetic field is applied during the oriented solidification process, so that the dendritic crystal is enabled to be affected by action of magnetizing force and leads an easy magnetization axis to incline to the field direction (namely the oriented solidification direction), and the alloy dendritic crystal orientation is controlled. The method is characterized in that a strong magnetostatic field with 1-14T (Tesla) is utilized, typical Bridgman oriented solidification device is adopted, a solid liquid interface of oriented solidification alloy is designed in a central steady area in the strong magnetostatic field, the entire orientated solidification process is completed under the strong magnetostatic field, an elongated alloy rod is utilized, and temperature gradient of a sample solid liquid interface changes along with furnace temperature and types of alloy. The drawing speed for downward oriented solidification of the alloy rod ranges from 5 to 100 micrometers/s, the dendritic crystal is immediately drawn into a cooling medium for quenching when growing to a stable stage, and finally the oriented solidification structure with the dendtritic crystal growing direction changed is obtained.
Description
Technical field
The present invention relates to a kind of method of high-intensity magnetic field control oriented freezing organization dendritic orientation, belong to alloy structure control studying technological domain.
Background technology
Dendrite is that material prepares a kind of style of organizing the most common in the forming process, and its size and form have very important impact to the final performance of material.Generally, the orientation of dendrite growth can be consistent with direction of heat flow as far as possible or opposite, and along the preferred orientation of being determined by crystallography grow (example: Al dendrite, preferentially dendritic orientation is＜100 〉; Sn dendrite, preferentially dendritic orientation is＜110 〉).In the dendrite monocrystalline (for example turbo blade) of directional solidification, all dendrites that form this single crystal grain are all fitly lined up, thereby have improved high-temperature behavior.
Because there are obvious anisotropy in oriented freezing organization and monocrystalline, the impact of crystal orientation alloy performance also is one of study hotspot.The people such as Dalal find that the enduring quality of monocrystalline SC7-14-6 alloy is with＜111〉when orientation be for the highest.Mckay etc. studies show that 760 ℃ of croop properties the Mar-M247 monocrystalline, in crystal orientation＜001〉and＜111〉direction higher performance is arranged all.Because high symmetrical crystal orientation (＜001 〉,＜111 〉), it is less that the crystal creep reaches the required Crystal Rotation of cross-slip, entered immediately for the second creep stage through the initial creep state of less, thereby generally have long creep rupture life.Above research shows that all the orientation of crystal in the oriented freezing organization directly affects the properties of material.So far, in order to obtain to have the material structure of certain dendritic orientation, the general means that adopt are by directional solidification seed crystal method control crystal orientation, or have the material of certain orientation texture by rolling acquisition.But the seed crystal method often need to prepare provide certain orientation monocrystalline as seed crystal, need to expend a large amount of human and material resources.By the material that milling method obtains, its texture degree of orientation is not high.
Summary of the invention
For the deficiency that prior art exists, the purpose of this invention is to provide a kind of method of high-intensity magnetic field control oriented freezing organization dendritic orientation.With seed crystal method and rolling contrast, this method is by introducing high-intensity magnetic field in the directional solidification process, and the crystal that high-intensity magnetic field will cause having magnetic anisotropy rotates, and causes easy axis to turn to magnetic direction.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method of high-intensity magnetic field control oriented freezing organization dendritic orientation has following process and step:
A. select 99.99% high purity alloys raw material, the configuration alloying component respectively is the Bi-0.85wt%Mn(Bi-Mn alloy), the Al-12wt%Ni(Al-Ni alloy), the Al-4.5wt%Cu(Al-Cu alloy) three kinds of alloy meltings in vacuum drying oven, electromagnetic agitation 1 hour, after making the abundant alloying of raw material, be that the quartz ampoule of 3mm carries out negative pressure of vacuum and inhales casting with internal diameter, obtain the alloy bar sample of the homogeneous chemical composition of the different Bi-Mn of dendritic growth preferred orientation and direction of easy axis, Al-Ni and three kinds of systems of Al-Cu, and it is encapsulated in the corundum crucible;
B. the conventional device for directionally solidifying of tradition is put into superconduction strong static magnetic field artificial body for generating, the static magnetic field strength scope that superconducting magnet produces is 1 ~ 14T; Corundum crucible is positioned on the pull bar of device for directionally solidifying, can be in heating furnace pull for vertical movement; Heating makes alloy melting, is incubated after 0.5 hour, opens the pull system and carries out directed pull with the pulling rate of setting; Sample directional solidification direction is parallel with magnetic direction, and the thermograde of forward position, freezing interface liquid phase changes with furnace temp; Heating furnace center furnace temperature is 650 ℃ in the alloy directionally solidified process of Bi-Mn, and the thermograde in solid liquid interface forward position is 50K/cm; The heating furnace center furnace temperature of Al-Ni and Al-Cu alloy is 900 ℃, and thermograde is respectively 38K/cm and 68K/cm; Guarantee that in the pull process solid liquid interface is in the steady magnetic field zone;
When c. pull is to stable growth, draws in rapidly in the Ga-In-Sn quenching bath and quench, obtain the directional solidification columanar structure that the dendritic growth direction changes.
The inventive method adopts the conventional device for directionally solidifying of tradition, comprises protective atmosphere input pipe, water cold sleeve, heating furnace, temperature regulating device, alloy bar sample, superconduction kicker magnet, quenching bath, corundum crucible and pull bar; The corundum crucible that is placed with the alloy bar sample is placed in the heating furnace; The outside of heating furnace is equipped with water cold sleeve, and the superconduction kicker magnet places the outside of water cold sleeve, and magnetic direction parallels with the directional solidification direction; Solid liquid interface places the steady zone of superconduction kicker magnet in the alloy directionally solidified process; Heating furnace connects temperature regulating device and controls its temperature; The one protective atmosphere input pipe that passes into inert gas is arranged on the heating furnace top; Pull bar is connected with corundum crucible; Quenching bath is positioned at the heating furnace below.
Principle of the present invention is based on has anisotropic crystal, can be orientated in magnetic field.Suppose that one has anisotropic crystal and is in the magnetic field, the magnetic moment of unit volume can be expressed as:
Wherein, θ is the angle of c-axis and magnetic direction, and when magnetic field changed, the energy of magnetization that is placed on magnetic anisotropy crystal was wherein changed into:
Formula (2) and formula (3) substitution formula (4) are got
Integration gets:
Will
Substitution formula (6):
Here
Be
cAxle and
AbAxial magnetization rate variance.
When
(8)
When
When
,
, this meaning c-axis directional steering magnetic field; On the contrary, when
, the ab direction of principal axis turns to magnetic field.More than can find out, put into its easy magnetizing axis of magnetic field when a paramagnetic magnetic anisotropy particle and turn to magnetic direction, and diamagnetic magnetic anisotropy particle is put into its easy magnetizing axis of magnetic field and turned on the plane perpendicular to magnetic direction.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and significant progressive:
This method is a kind of new method that changes the oriented freezing organization dendritic orientation by controlling magnetic field intensity and directional solidification speed, the present invention applies axial high-intensity magnetic field in alloy directionally solidified process, discovery is for the directional solidification preferential growth direction crystal different from the crystal direction of easy axis, and applying of magnetic field causes the arborescent structure orientation to change.This method be as long as applying magnetostatic field at present industrial widely used high speed clotting method just can achieve the goal, and is simple to operate and be easy to realization.
Description of drawings
Fig. 1 is that Bridgman is legal to the coagulation system schematic diagram under the conventional high-intensity magnetic field of the tradition utilized of the present invention.
Fig. 2 is the principle schematic of the inventive method, wherein (a) and (b) and (c) be respectively the crystal easy axis parallel with the preferential growth direction, have in certain angle and the vertical three kinds of situations, apply high-intensity magnetic field to the effect of dendritic growth orientation.
Fig. 3 is respectively the different alloy of Bi-0.82wt%Mn, Al-4.5wt%Cu and three kinds of primary phase dendrite of Al-12wt%Ni performance at the tissue that has or not the directional solidification longitudinal section under the strong magnetic field action.
The specific embodiment
After below in conjunction with accompanying drawing specific embodiments of the invention being described in.
Implementing material selection primary phase is the Bi-0.82wt%Mn alloy of MnBi crystal.According to the pure Bi of alloy ratio weighing and pure Mn metal, in vacuum drying oven, carry out melting.After the electromagnetic agitation 1 hour, be that the quartz ampoule of 3mm carries out negative pressure and inhales casting with internal diameter, obtain the alloy bar of homogeneous chemical composition, and it is encapsulated in the alundum tube.Alundum tube is contained on the pull bar, and pull bar connects the servo pull of directional solidification system.Design makes the solid liquid interface of sample be in kicker magnet steady magnetic field zone, and device for directionally solidifying is typical Bridgman device.The pulling rate of servo pull system setting is that 5 μ m/s, thermograde are 50K/cm, are to carry out directional solidification under the 10T in magnetic field intensity.The sample of directional solidification reaches the stable growth zone behind pull 8cm, at this moment draw in rapidly in the Ga-In-Sn quenching bath with a larger pulling rate and quench.Directional solidification sample symmetrical incision below solid liquid interface with gained obtains the longitudinal section sample of tissues observed, behind the inlaying samples, through grinding, polish the post-etching tissues observed.
The process of the present embodiment and step and above-described embodiment 1 are basic identical.Special feature is: the alloy of employing is Al-4.5wt%Cu, and primary phase is α-Al.The directional solidification drawing velocity is 50 μ m/s, and heating furnace central area temperature is 900 ℃, and thermograde is 38K/cm.
The process of the present embodiment and step and above-described embodiment 1 are basic identical.Special feature is: the alloy of employing is Al-12wt%Ni, and primary phase is Al
3Ni.The directional solidification drawing velocity is 100 μ m/s, and heating furnace central area temperature is 900 ℃, and thermograde is 68K/cm, and magnetic field intensity is 12T.
Three embodiment selected respectively the preferential growth direction identical with direction of easy axis, exist certain angle and vertical three kinds of crystal as research object.What Fig. 2 showed is respectively that the schematic diagram that the effect in magnetic field causes the growth of dendrite to change, solid arrow represent the preferential growth direction of crystal in above-mentioned three kinds of situations, and dotted arrow represents the easy axis of crystal.For the preferential growth direction MnBi primary phase identical with direction of easy axis, the electromagnetic force that crystal is subject under magnetic field will induce MnBi to grow along magnetic direction; For the Al-4.5wt%Cu alloy, its primary phase dendrite is α-Al, and its preferential growth direction is＜100 〉, its direction of easy axis is＜111 〉, under the effect in magnetic field, dendrite will deflect, direction of easy axis＜111〉arrange along the directional solidification direction.For Al-12wt%Ni alloy, primary phase Al
3The preferential growth direction of Ni is vertical with direction of easy axis, and the dendrite of this alloy is under the effect in magnetic field, and its direction of growth can be perpendicular to magnetic direction.Fig. 3 is the longitudinal section oriented freezing organization photo of above-mentioned three embodiment.
In the directional solidification process under magnetic field, having anisotropic crystal will grow along its preferred orientation direction, but the easy magnetizing axis of crystal will turn to magnetic direction simultaneously.When easy axis is identical with the preferential growth direction, axial magnetic field will improve the growth of directional solidification direction.Among the embodiment 1, the MnBi crystal＜001〉direction to be not only easy axis also be the preferential growth direction, so applying of magnetic field can promote dendrite along the growth of directional solidification direction in the directional solidification process.Among the embodiment 2, in the Al-4.5wt%Cu alloy, the easy axis of Al crystal and preferential growth direction be respectively＜111〉and＜100〉direction, therefore under the 10T magnetic fields, Al crystal＜111〉directional steering directional solidification direction.Under special circumstances, such as embodiment 3, Al
3Ni crystal easy magnetizing axis and preferred orientation perpendicular direction, the effect in magnetic field cause the preferential growth perpendicular direction in the directional solidification direction, have formed layer structure.
Claims (1)
1. the method for high-intensity magnetic field control oriented freezing organization dendritic orientation is characterized in that having following process and step:
A. select 99.99% high purity alloys raw material, the configuration alloying component respectively is: Bi-Mn alloy: Bi-0.85wt%Mn, Al-Ni alloy: Al-12wt%Ni, three kinds of alloy meltings in vacuum drying oven of Al-Cu alloy: Al-4.5wt%Cu, electromagnetic agitation 1 hour, after making the abundant alloying of raw material, be that the quartz ampoule of 3mm carries out negative pressure of vacuum and inhales casting with internal diameter, obtain the alloy bar sample of the homogeneous chemical composition of the different Bi-Mn of dendritic growth preferred orientation and direction of easy axis, Al-Ni and three kinds of systems of Al-Cu, and it is encapsulated in the corundum crucible that internal diameter is 3mm;
B. device for directionally solidifying is put into superconduction strong static magnetic field artificial body for generating, the static magnetic field strength scope that superconducting magnet produces is 1 ~ 14T; Corundum crucible is positioned on the pull bar of device for directionally solidifying, can be in heating furnace pull for vertical movement; Heating makes alloy melting, is incubated after 0.5 hour, opens the pull system and carries out directional solidification with the pulling rate speed of setting, and withdrawing rate is 5 ~ 100 μ m/s; Sample directional solidification direction is parallel with magnetic direction, and the thermograde of forward position, freezing interface liquid phase changes with furnace temp; Heating furnace center furnace temperature is 650 ℃ in the alloy directionally solidified process of Bi-Mn, and the thermograde in solid liquid interface forward position is 50K/cm; The heating furnace center furnace temperature of Al-Ni and Al-Cu alloy is 900 ℃, and thermograde is respectively 38K/cm and 68K/cm; Guarantee that in the pull process solid liquid interface is in the steady magnetic field zone;
When c. pull is to stable growth, draws in rapidly in the Ga-In-Sn quenching bath and quench, obtain the directional solidification arborescent structure that the dendritic growth direction changes.
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| CN103233272A (en) * | 2013-05-08 | 2013-08-07 | 上海大学 | Method for phase separation of original ecological microcrystals in Bi-Mn alloy by using stereospecific polymerization |
| CN103990780A (en) * | 2014-05-19 | 2014-08-20 | 上海大学 | Method for manufacturing gradient materials under transverse magnetic field and directional solidification device |
| CN104416252A (en) * | 2013-08-28 | 2015-03-18 | 中国科学院金属研究所 | Preparation method of preferred orientation texture welding spots |
| CN104625022A (en) * | 2015-01-23 | 2015-05-20 | 上海大学 | Method for purifying impurities in metal through directional solidification under transverse magnetic field |
| CN104862777A (en) * | 2015-05-19 | 2015-08-26 | 上海大学 | Method and device for controlling crystal orientation in steady-state magnetic field through directional solidification |
| CN105195716A (en) * | 2015-09-24 | 2015-12-30 | 上海大学 | Method for conducting oriented solidification on CET refining metal solidification organization under longitudinal magnetic field |
| CN107537994A (en) * | 2017-08-28 | 2018-01-05 | 上海大学 | The method that magnetic field auxiliary directional solidification prepares strong-texture polycrystalline magnetically controlled shape memory material |
| CN108655375A (en) * | 2018-05-17 | 2018-10-16 | 上海大学 | The method and its device for directionally solidifying of functionally graded material are prepared using axial homogeneous magnetic field |
| CN108728678A (en) * | 2018-05-03 | 2018-11-02 | 北京科技大学 | A kind of iron-based superconductor preparation method based on isostatic cool pressing and directional solidification technique |
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| CN104416252A (en) * | 2013-08-28 | 2015-03-18 | 中国科学院金属研究所 | Preparation method of preferred orientation texture welding spots |
| CN104416252B (en) * | 2013-08-28 | 2016-08-10 | 中国科学院金属研究所 | A kind of preparation method of preferred orientation texture solder joint |
| CN103990780A (en) * | 2014-05-19 | 2014-08-20 | 上海大学 | Method for manufacturing gradient materials under transverse magnetic field and directional solidification device |
| CN104625022A (en) * | 2015-01-23 | 2015-05-20 | 上海大学 | Method for purifying impurities in metal through directional solidification under transverse magnetic field |
| CN104625022B (en) * | 2015-01-23 | 2017-08-11 | 上海大学 | A kind of method of field trash in transverse magnetic field directional solidification purification metal |
| CN104862777A (en) * | 2015-05-19 | 2015-08-26 | 上海大学 | Method and device for controlling crystal orientation in steady-state magnetic field through directional solidification |
| CN104862777B (en) * | 2015-05-19 | 2018-03-02 | 上海大学 | The method and device of directional solidification control crystal orientation under steady magnetic field |
| CN105195716B (en) * | 2015-09-24 | 2018-07-10 | 上海大学 | The method of directional solidification CET thinning metal solidification textures under longitudinal magnetic field |
| CN105195716A (en) * | 2015-09-24 | 2015-12-30 | 上海大学 | Method for conducting oriented solidification on CET refining metal solidification organization under longitudinal magnetic field |
| CN107537994A (en) * | 2017-08-28 | 2018-01-05 | 上海大学 | The method that magnetic field auxiliary directional solidification prepares strong-texture polycrystalline magnetically controlled shape memory material |
| CN108728678A (en) * | 2018-05-03 | 2018-11-02 | 北京科技大学 | A kind of iron-based superconductor preparation method based on isostatic cool pressing and directional solidification technique |
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Application publication date: 20130424 |